Process for the preparation of high-purity zirconium, hafnium, tantalum and niobium alkoxides
View Patent ↗A novel process for the preparation of high-purity zirconium, hafnium, tantalum and niobium alkoxides (alcoholates), novel tantalum and niobium compounds and a process for their preparation are provided. The process comprises the steps of mixing crude metal alkoxides M(OR) x having a halogen impurity of at least 0.05 wt. %, with an alcohol ROH, in which R is a C 1 -C 12 -alkyl radical, and subsequently or simultaneously metering in an excess of ammonia, based on the amount of mononuclear or polynuclear halogen-containing metal alkoxides.
1. Process for the preparation of high-purity metal alkoxides M(OR) x , in which M is Nb, Ta, Zr or Hf, x is 5 in the case of M=Nb or Ta and 4 in the case of M=Zr or Hf, and R independently of one another are identical or different C 1 -C 12 -alkyl radicals, wherein
(a) a crude metal alkoxide product M(OR) x with a halogen content of >200 ppm, containing as impurity at least 0.05 wt. % of mononuclear or polynuclear halogen-containing metal alkoxides, is mixed with
(b) at most 30 wt. % based on the total amount of crude alkoxide, of an alcohol ROH, in which R is a C 1 -C 12 -alkyl radical, and
(c) subsequently or simultaneously an excess of ammonia, based on the amount of mononuclear or polynuclear halogen-containing metal alkoxides, based on the total amount of crude alkoxide, is metered in.
2. Process according to claim 1 , wherein M is Ta or Nb and the mononuclear or polynuclear halogen-containing metal alkoxide present as impurity is the compound M 2 (OR) 9 Hal, in which Hal is F, Cl, Br or I and R is as defined in claim 1 .
3. Process according to claim 1 , wherein M is Zr or Hf and the mononuclear or polynuclear halogen-containing metal alkoxide(s) present as impurity is (are) at least one compound M p (OR) 4p−q Hal q , in which Hal is F, Cl, Br or I, q is 1, 2, 3 or 4, p is 2, 3 or 4 and R is as defined in claim 1 .
4. Process according to claim 1 , wherein the radical R is C 1 -C 5 -alkyl and Hal is Cl.
5. Process according to claim 1 , wherein the radical OR is an ethoxy group and M is Ta.
6. A compound of the formula M 2 (OR) 9 Hal in which R is as defined in claim 1 , M is Ta or Nb and Hal is a halogen from the group comprising F, Cl, Br and I.
7. A compound of the formula M 2 (OR) 9 Hal according to claim 6 in which R is a C 1 -C 5 -alkyl radical and Hal is Cl.
8. A compound according to claim 7 , wherein it is Ta 2 (OEt) 9 Cl.
9. Mixtures of compounds M 2 (OR) 9 Hal according to claim 6 and M(OR) 5 containing at least 0.05 wt. % of M 2 (OR) 9 Hal.
10. Mixtures according to claim 9 in which R is a C 1 -C 5 -alkyl radical and Hal is Cl.
11. Mixtures according to claim 9 consisting of Ta 2 (OEt) 9 Cl and Ta(OEt) 5 .
12. Process according to claim 1 , wherein the halogen content is from 0.1 to 10.0 wt. %.
13. Process according to claim 1 , wherein the amount of alcohol ROH is from 4 to 12 wt. %.
14. Process according to claim 1 , wherein the amount of ammonia is between 0.1 to 5.0 wt. %.